Caracterización del zumo de limón español

(Citrus limon (L.) Burm.) y valorización de

subproductos industriales

José Lorente Fernández

http://hdl.handle.net/10803/664901

ADVERTIMENT. L'accés als continguts d'aquesta tesi doctoral i la seva utilització ha de respectar els drets
de la persona autora. Pot ser utilitzada per a consulta o estudi personal, així com en activitats o materials
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(RDL 1/1996). Per altres utilitzacions es requereix l'autorització prèvia i expressa de la persona autora. En
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persona autora i el títol de la tesi doctoral. No s'autoritza la seva reproducció o altres formes d'explotació
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ADVERTENCIA. El acceso a los contenidos de esta tesis doctoral y su utilización debe respetar los
derechos de la persona autora. Puede ser utilizada para consulta o estudio personal, así como en
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Refundido de la Ley de Propiedad Intelectual (RDL 1/1996). Para otros usos se requiere la autorización
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ventana o marco ajeno a TDR (framing). Esta reserva de derechos afecta tanto al contenido de la tesis como
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WARNING. Access to the contents of this doctoral thesis and its use must respect the rights of the author. It
can be used for reference or private study, as well as research and learning activities or materials in the
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or frame external to TDX (framing) is not authorized either. These rights affect both the content of the thesis
and its abstracts and indexes.



 




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 Universitat de Lleida
Departament Tecnologia d’Aliments
Av. Alcalde Rovira Roure, 191
25198 Lleida
Tel.: (+34 973 702521 / 973 702500
Fax :(+34 973 702596
dta@tecal.udl.es

El Dr. Albert Ibarz Ribas, Catedrático de Universidad del Área de Tecnología de Alimentos del
Departamento de Tecnología de Alimentos de la Universidad de Lleida y la Dra. Nuria Martí
Bruñá, Profesor Contratado Doctor del Área de Tecnología de Alimentos del Departamento de
Tecnología de Agroalimentaria de la Universidad Miguel Hernández

Hacen constar:

Que la Tesis Doctoral titulada “Caracterización del zumo de limón español (Citrus limon
(L.) Burm.) y valorización de subproductos industriales”, de la que es autor José Lorente,
ha sido realizada bajo su dirección, su contenido se corresponde con el proyecto de tesis
aprobada en su momento y cumple las condiciones requeridas para optar al grado de Doctor por
la Universidad de Lleida. Por todo ello,

Autorizan:

A que esta memoria se presente para su defensa oral.

Lleida y Orihuela, 8 de octubre de 2015

Fdo: Albert Ibarz Ribas Fdo: Nuria Martí Bruñá











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ROWTYPE_ LEVEL_ VARNAME_ DIM1 DIM2 DIM3 DIM4

QUANT CORE Parte -0,693 -0,527 0,347 -0,152
QUANT FRIT Parte -0,173 0,434 0,125 0,579
QUANT PIEL Parte 0,865 0,093 -0,473 -0,427
QUANT Valencia Late Almería Variedad -0,456 0,426 0,439 -1,241
QUANT Valencia Late Murcia Variedad -0,611 0,361 -1,06 0,313
QUANT Lane Late Variedad 0,406 0,192 -0,124 0,304
QUANT Limón Fino Variedad 0,661 -0,979 0,745 0,625
QUANT Método 1 Metodo 0,19 0,569 0,417 0,05
QUANT Método 2 Metodo -0,19 -0,569 -0,417 -0,05
QUANT Retención muy baja de aceite Aceite -0,081 -0,227 -0,918 -0,101
QUANT Retención baja de aceite Aceite 0,449 0,391 -0,108 0,195
QUANT Retención alta de aceite Aceite -0,368 -0,164 1,026 -0,094
QUANT Retención muy baja de agua Agua -1,111 -0,295 0,016 0,155
QUANT Retención baja de agua Agua 0,252 -0,465 -0,048 -0,09
QUANT Retención alta de agua Agua 0,859 0,76 0,032 -0,066
QUANT Cerca del blanco absoluto ColorL -0,634 0,559 0,053 0,191
QUANT Lejos del blanco absoluto ColorL 0,634 -0,559 -0,053 -0,191
QUANT Mucho más verde que óptimo Colora -0,959 0,694 0,248 0,015
QUANT Más verde que óptimo Colora 0,492 0,309 -0,05 -0,412
QUANT Verde cercano a óptimo Colora 0,467 -1,003 -0,198 0,397
QUANT Menos amarillo que óptimo Colorb -0,05 -0,426 0,565 0,364
QUANT Amarillo cercano a óptimo Colorb -0,447 0,414 0,142 0,57
QUANT Más amarillo que óptimo Colorb 0,497 0,012 -0,708 -0,935
QUANT Menos rendimiento que óptimo Rendimie 0,224 0,509 -0,153 0,811
QUANT Rendimiento medio Rendimie -0,239 -0,989 -0,303 0,148
QUANT Más rendimiento que óptimo Rendimie 0,015 0,48 0,455 -0,959
QUANT óptimo Viscosid -0,942 -0,355 0 -0,247
QUANT Viscosidad más baja óptimo Viscosid 0,053 0,225 -0,665 -0,018
QUANT Viscosidad cerca de óptimo Viscosid 0,889 0,13 0,665 0,265
QUANT Degradación alta Estructu -1,251 0,07 -0,603 0,041
QUANT Degradación media Estructu 0,193 -0,326 0,457 -0,289
QUANT Fibra sin degradació Estructu 0,998 0,763 -0,466 0,701
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CORE 239,86 139,07 60,36 11,5 450,8

FRIT 14,92 94,26 7,85 167,68 284,71
PIEL 374,43 4,34 111,74 91,37 581,88
Valencia Late almeri 69,32 60,36 64,11 513,26 707,05
Valencia Late murcia 124,26 43,55 374,46 32,56 574,83
Lane Late 54,83 12,29 5,1 30,74 102,96
Limón fino 145,65 319,48 185,03 130,06 780,22
Método 1 36,27 323,28 173,7 2,54 535,8
Método 2 36,27 323,28 173,7 2,54 535,8
Retención muy baja de aceite 3,31 25,73 421,51 5,14 455,69
Retención baja de aceite 100,99 76,32 5,85 19,11 202,27
Retención alta de aceite 67,74 13,42 526,64 4,43 612,23
Retención muy baja de agua 616,8 43,48 0,13 12,07 672,48
Retención baja de agua 31,64 108,2 1,14 4,03 145
Retención alta de agua 369,06 288,85 0,5 2,15 660,56
Cerca del blanco absoluto 401,65 312,53 2,83 36,32 753,32
Lejos del blanco absoluto 401,65 312,53 2,83 36,32 753,32
Mucho más verde que óptimo 459,84 240,89 30,66 0,12 731,51
Más verde que óptimo 121,16 47,76 1,23 84,96 255,11
Verde cercano a óptimo 108,92 503,15 19,63 78,77 710,47
Menos amarillo que óptimo 1,26 90,76 159,81 66,38 318,2
Amarillo cercano a óptimo 99,81 85,77 10,13 162,68 358,39
Más amarillo que óptimo 123,47 0,07 250,39 436,89 810,82
Menos rendimiento que óptimo 25,04 129,55 11,64 328,66 494,9
Rendimiento medio 28,58 489,07 45,76 10,94 574,34
Más rendimiento que óptimo 0,12 115,19 103,57 459,5 678,38
Viscosidad muy por debajo de 443,48 62,94 0 30,41 536,84
Viscosidad más baja óptimo 1,39 25,29 220,84 0,17 247,68
Viscosidad cerca de óptimo 395,27 8,44 220,8 35,08 659,59
Degradación alta 521,38 1,65 121,14 0,57 644,74
Degradación media 44,17 125,5 247,29 98,46 515,42
Fibra sin degradació 262,18 153,14 57,13 129,24 601,69

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 Food Chemistry 162 (2014) 186–191

Contents lists available at ScienceDirect

Food Chemistry
journal homepage: www.elsevier.com/locate/foodchem

Chemical guide parameters for Spanish lemon (Citrus limon (L.) Burm.)
juices
José Lorente a, Salud Vegara a, Nuria Martí a, Albert Ibarz b, Luís Coll c, Julio Hernández c,
Manuel Valero a,⇑, Domingo Saura a
a
IBMC-JBT Corp., FoodTech R&D Alliance, Instituto de Biología Molecular y Celular, Universidad Miguel Hernández (UMH) – Campus de Orihuela, Carretera de Beniel km 3.2, 03312
Orihuela, Alicante, Spain
b
Departament de Tecnologia d’Aliments UPV-XaRTA, Universitat de Lleida, Av. Rovira Roure, 191, 25198 Lleida, Spain
c
Laboratorios ECOSUR S.A., Calle Castillo de Aledo s/n, Polígono Industrial Base 2000 – San Martín, 30564 Lorquí, Murcia, Spain

a r t i c l e i n f o a b s t r a c t

Article history: To contribute for setting reference guideline for commercial juice extracted from the Spanish lemon
Received 3 March 2014 varieties, chemical composition of 92 direct and 92 reconstituted samples were investigated. In direct
Received in revised form 8 April 2014 lemon juice, titratable acidity was 52.4 g/L, being the citric acid the main component. Glucose, fructose
Accepted 10 April 2014
and sucrose concentrations were 7.9, 7.3 and 4.5 g/L, respectively. Predominant mineral was potassium
Available online 21 April 2014
(1264.2 mg/L), followed by phosphorous (306 mg/L), calcium (112 mg/L) and magnesium (92.6 mg/L).
Hesperidin ranged from 257 to 484.8 mg/L, while water soluble pectins varied between 164.8 and
Keywords:
550 mg/L. Similar values were obtained in reconstituted lemon juice. There are different parameters that
Lemon juice
Reference guideline
did not reach or exceeded the limits proposed by the European Association of the Industry of Juices and
Chemical composition Nectars. These levels should be taken into account to modify the present reference guideline and that
Organic acids Spanish lemon juices are not discarded for to have lower or bigger values.
Sugar profile Ó 2014 Elsevier Ltd. All rights reserved.
Hesperidin content

1. Introduction
Lemon fruit (Citrus limon (L.) Burm.) is also a rich source of
nutrients, including flavonoids, citric acid, vitamin C and minerals
(e.g. potassium), which provide numerous health promoting
properties (Del Río et al., 2004; Gil-Izquierdo, Riquelme, Porras, &
Ferreres, 2004; González-Molina, Moreno, & García-Viguera,
2008, 2009a).
Lemon production is limited to a small number of countries
and regions because of the plant’s extreme sensitivity to low
temperatures. In Spain (the main lemon producing country in the
Mediterranean area), the crop is concentrated in the Region of
Murcia and in some neighbouring provinces of Alicante (Valencian
Community) and Almería (Andalusia). In Murcia Region, lemon
production is dominated by the autochthonous ‘Fino’ and ‘Verna’
varieties followed by the foreign varieties ‘Eureka’, originated in
California (USA), and ‘Lisbon’ from Portugal (Pérez-Pérez, Castillo,
García-Lidón, Botía, & García-Sánchez, 2005). The ‘Verna’ lemon
produces good-sized fruits and good juice content with not many
⇑ Corresponding author. Tel.: +34 96 674 96 83; fax: +34 96 674 96 19.
E-mail address: m.valero@umh.es (M. Valero).
seeds and the ‘Fino’ lemon, is smaller than the ‘Verna’, with a
high-yield extraction of juice.
The levels of different compounds vary in juices prepared from
different lemon cultivars, maturity stage, growing region, cultural
practise, storage conditions of fruits, extraction procedure and
thermal treatment of juice.
There are two different kinds of lemon juices on the market:
Not From Concentrate (NFC), obtained by simple squeezing of the
fruit and then submit it to a mild pasteurisation, and From Concen-
trate Juice (FCJ) obtained by reconstituting concentrate fruit juice
up to the original characteristics of the juice. Obtaining fruit juice
concentrates through water reduction in the original juice shows
some advantages in the product: higher resistance to microbes
and chemical deterioration as a result of water activity reduction
and volume and weight reduction with consequent reduction of
transport, storage and packaging costs.
The industrial concentration of fruit juices is usually performed
by thermal evaporators, in which much more drastic temperature
and time regimes than pasteurisation process can be used
(Bánvölgyia, Horvátha, Stefanovits-Bányaib, Békássy-Molnára, &
Vataia, 2009; Onsekizoglu, Bahceci, & Acar, 2010). It is known that
the thermal treatment by pasteurisation and/or thermal concentra-
tion produces modifications of some components with consequent

http://dx.doi.org/10.1016/j.foodchem.2014.04.042
0308-8146/Ó 2014 Elsevier Ltd. All rights reserved.
 J. Lorente et al. / Food Chemistry 162 (2014) 186–191
degeneration of taste and chemical characteristics (Marín,
Martínez, Uribesalgo, Castillo, & Frutos, 2002).
The AIJN, Association of the Industry of Juices and Nectars of the
European Union (EU), has established reference guidelines for sev-
eral fruit juices, including lemon. The referred values in these
guidelines are based on pure, authentic fruit juices obtained from
the edible part of mature and sound fruits of different varieties
and geographical origins obtained by mechanical processes. The
characterisation of Spanish lemon juices by measuring their phys-
icochemical quality parameters is of special interest to contrast
them with the actual international standards: Codex Alimentarius
and AIJN Code of practises. It is also very useful to detected adulte-
ration or dilution of juices and to distinguish these high-quality
juices.
The aim of this study was to contribute to the knowledge of
Spanish lemon juice characteristics, obtained from edible part of
Spanish fruits, from varieties ‘Verna’ and ‘Fino’ and compare the
effects of concentration process in the nutritional quality of lemon
juices. The obtained parameters will be compared with the inter-
national standards and will serve to change them, if necessary.
2. Materials and methods
2.1. Materials
Two typical lemon varieties cultivated in Murcia (South-Eastern
Spain) were selected for this research: ‘Verna’ and ‘Fino’. Lemons
were provided by different local factories of citrus juice extraction
and processing. They were processed at the Miguel Hernández Uni-
versity Pilot Plant, which is part of IBMC-JBT Corp., FoodTech R&D
Alliance, for juice extraction. A cleaned JBT FoodTech Citrus Juice
Extractor (juicer) was used to obtain lemon juice. The extractor
separates the juice from those constituents which, if allowed to
remain in contact with the juice for any period of time, will have
an adverse effect on the end product. After that, juice and sus-
pended pulp were separated in a citrus finisher and only 8–12%
of precipitable pulp was present.
Ninety-two (92 samples) pulp-free lemon juices were concen-
trated in a falling film evaporator (Inoxpaser, Molina de Segura,
Murcia, Spain) with a feed flow of 100 L/h and adiabatic vacuum
effect. The evaporator removes most of the water until the juice
attains a high concentration of sugars (65°Brix).
Samples were collected for three different campaigns
(2002–2003, 2003–2004, 2004–2005) and were analysed in dupli-
cate following the methods described below.
2.2. Analytical reference methods
A panel of different analytical techniques established by IFU
(International Federation of Fruit Juice Producers, Paris, France)
was used for determination of physicochemical parameters,
organic and mineral contents in lemon juices.
Brix value was measured according to the IFU method (8) and
titratable acidity according to IFU method (3). Relative density
20/20 in lemon juices was determined with IFU method (1). Enzy-
matic methods established by IFU (54, 21, 64, 17a, 22) were used
for determination of D-isocitric, L-malic, D-malic, L-ascorbic and cit-
ric acid contents. Lactic acid was determined with enzymatic
method (IFU 53), ethanol with IFU 52 and volatile acids according
to IFU method (5). Glucose, fructose and sucrose con tents were
determined according to enzymatic method established by IFU
(55, 56). Formol index was determined according to the method
established by IFU (30) and calculated as mL 0.1 N NaOH/100 mL
fruit juice. Amino acid profile was determined according to IFU
method 57. Sodium, potassium, magnesium and calcium contents
187
were determined with the IFU method (33) and ash with IFU
method number 9. Arsenic and heavy metals were determined
by atomic absorption spectrometry (AAS). Total phosphorus and
sulphate were determined according IFU 50 and 36. The content
of water soluble pectin, hesperidin, D-sorbitol and 5-hydroxymeth-
ylfurfural (5-HMF) were determined with IFU methods 26, 58, 62
and 69, respectively.
2.3. Statistical procedure
Hundred eighty-four (184) direct and reconstituted juice sam-
ples from the Spanish lemon varieties ‘Verna’ and ‘Fino’ were ana-
lysed in duplicate following the IFU methods. There was large
variability in the values of constituents of pure juice due to genetic,
environmental, and maturational differences among samples of
juice. This heterogeneity of samples affects all statistical methods
of quality control of juice (Brown, Katz, & Cohen, 1988). As it has
been reported for pomegranate juice database (Vegara et al.,
2014), the means and the standard deviations (SD) for many tested
characteristics of the lemon juice were calculated and the corre-
sponding variation intervals were compared with the permissible
limits adopted by AIJN.
3. Results and discussion
3.1. Section A: Parameters that characterise the absolute quality
requirements
Results related to compositional, environmental, hygienic, and
industrial requirements of direct and reconstituted lemon juices
are listed in Tables 1 and 2, respectively. According to these results,
relative densities for direct and reconstituted juice were 1.03155
and 1.0177, respectively. A 23.5% of results for direct juices are
lower than the AIJN proposal levels and a 76.5% are higher. Also
the reconstituted juices differ in density, with a 30.8% of values
below the minimum proposal and a 67% above.
Total soluble solids (TSS) of direct lemon juices ranged from 5 to
10.5°Brix and presented lower and higher values than those estab-
lished by AIJN (2013). According to González-Molina, Moreno, and
García-Viguera (2009b), TSS in ‘Verna’ lemon juices was detected
in a concentration of 6–7.5°Brix and in ‘Fino’ variety between 8.2
and 9.5°Brix (García-Sánchez, Carvajal, Porras, Botía, & Martínez,
2003). Also, in the study of Marín et al. (2002) TSS were around
6.5–9.2°Brix. The results obtained in either these studies and in
the present show that Spanish lemons have TSS values higher than
those proposed by AIJN (2013). In FCJ, TSS is 8°Brix because it is a
reconstituted juice.
Other environmental, hygienic, and industrial requirements are
inside the range of values established in the reference guideline
(AIJN, 2013) and were not found differences between direct and
reconstituted juices. Thus, L-ascorbic acid presented a concentra-
tion of 408.1 and 403.6 mg/L in direct and reconstituted juices,
respectively. These results are bigger than others obtained for dif-
ferent authors in Spanish lemon juices (González-Molina et al.,
2008, 2009a, 2009b; Marín et al., 2002) and Chinese lemons (Xu
et al., 2008). The L-ascorbic content is subjected to variations
depending on variety, ripeness, processing, and storage conditions.
According to AIJN (2013), the natural L-ascorbic content in direct
lemon juice is, as rule, over 300 mg/L.
Heavy metal elements contained in fertiliser and contaminated
soils are transmitted into fruits and other farm products. Examples
of heavy metals that are harmful (causing serious health effects) to
humans include arsenic (As), lead (Pb), mercury (Hg), cadmium
(Cd) and chromium (Cr) (Vegara et al., 2014). Heavy metal contents
188 J. Lorente et al. / Food Chemistry 162 (2014) 186–191

Table 1
Absolute quality requirements that are considered as being mandatory for direct lemon juices marketed in the EU.

Unit Mean ± SD Range of variation AIJN proposal Values outside (%)

m M
1. Industrially agree upon requirements
Rel. density 20/20 – 1.03155 ± 0.01 1.0013–1.0612 1.0277 23.53 76.47
Corresponding Brix °Brix 7.8 ± 1.0 5–10.5 7 8.79 78.02
2. Hygiene requirements
Volatile acids as acetic acid g/L 0.1 ± 0.01 0–0.4 Max. 0.4
Ethanol g/L ND Max. 3.0
D/L Lactic acid g/L ND Max. 0.2

3. Environmental requirements
Arsenic and heavy metals
Arsenic (As) mg/L <0.005 Max. 0.1
Lead (Pb) mg/L <0.01 Max. 0.05
Mercury (Hg) mg/L <0.01 Max. 0.01
Cadmium (Cd) mg/L <0.01 Max. 0.05
4. Compositional requirements
L-Ascorbic
acid mg/L 408.1 ± 108.7 154.2–667.0 Min. 150
5-Hydroxymethylfurfural (5-HMF) mg/L 0.54 ± 0.02 0–5 Max. 20

SD, standard deviation; AIJN, Association of the Industry of Juices and Nectars of the European Union (EU); ND, not detectable; m, minimum; M, maximum.

Table 2
Absolute quality requirements that are considered as being mandatory for reconstituted lemon juices marketed in the EU.

Unit Mean ± SD Range of variation AIJN proposal Values outside (%)

m M
1. Industrially agree upon requirements
Rel. density 20/20 – 1.1222 ± 0.10 1.0177–1.3821 1.0318 30.77 67.03
Corresponding Brix °Brix 8 ± 1.0 8
2. Hygiene requirements
Volatile acids as acetic acid g/L 0.1 ± 0.01 0–0.4 Max. 0.4
Ethanol g/L ND Max. 3.0
D/L Lactic acid g/L ND Max. 0.2

3. Environmental requirements
Arsenic and heavy metals
Arsenic (As) mg/L <0.005 Max. 0.1
Lead (Pb) mg/L <0.01 Max. 0.05
Mercury (Hg) mg/L <0.01 Max. 0.01
Cadmium (Cd) mg/L <0.01 Max. 0.05
4. Compositional requirements
L-Ascorbic
acid mg/L 403.6 ± 114.0 175.1–774.7 Min. 150
5-Hydroxymethylfurfural (5-HMF) mg/L 0.71 ± 0.05 0–5 Max. 20

SD, standard deviation; AIJN, Association of the Industry of Juices and Nectars of the European Union (EU); ND, not detectable; m, minimum; M, maximum.

detected in all direct and reconstituted lemon juice samples by AAS
were acceptable (AIJN, 2013).
5-HMF is practically not present in direct fruit juice, but it is
naturally generated during heating or storage processes in the
Maillard reaction as well as sugar caramelization and degradation
(Vegara et al., 2014). Therefore, 5-HMF can be used as an indicator
of thermal abuse and prolonged or improper storage (Arena,
Fallico, & Maccarone, 2001; Esteve, Frígola, Rodrigo, & Rodrigo,
2005). In all lemon juice samples tested, concentration of 5-HMF
was much lower than 20 mg/L, the maximum prescribed value
by AIJN (2013). The limited presence of 5-HMF (0.54–0.71 mg/L)
is in agreement with the lack of heat treatment of the juices and
suitable preservation of the samples as is confirmed by the high
L-ascorbic acid content (Burdurlu, Koca, & Karadeniz, 2006).
3.2. Section B: Criteria relevant to the evaluation of identity and
authenticity
Chemical composition of hundred eighty-four (184) direct and
reconstituted juice samples from Spanish lemons are given in
Tables 3 and 4. According to these results, titratable acidity (TA)
of lemon juices, calculated as anhydrous citric acid (ACA) pH 8.1,
varied from 35.1 to 65.6 g/L in direct juices and from 38.4 to
78.1 g/L in reconstitutes. These values are similar than other values
obtained by different authors for Spanish and Chinese lemons
(García-Sánchez et al., 2003; Pérez-Pérez et al., 2005; Xu et al.,
2008).
Citric acid was the predominant organic acid component and its
amount ranged from 35.1 to 84.2 g/L and from 34.2 to 67.4 g/L in
direct and reconstituted juices, respectively. It was followed by
L-malic acid in a range of 0.5–5.0 g/L in both types of juice. D-Isocit-
ric acid was present in a concentration of 268.9 mg/L in direct
juices and at 258.7 mg/L in reconstitutes. The 35.2% and 42.9% of
results for D-isocitric acid in direct and reconstituted juices were
lower than the minimum limit proposed by AIJN (2013). The con-
centration of citric acid correlates with the isocitric acid concentra-
tion to a certain extent. The citric acid/isocitric acid ratio, therefore,
can be used to detect an acidification with citric acid. Usually the
ratio lies between 100 and 200 but values up to 240 can be
observed in Argentinean lemon juices (AIJN, 2013). In the present
 J. Lorente et al. / Food Chemistry 162 (2014) 186–191 189

Table 3
Other quality parameters and further criteria for evaluation of identity and authenticity of direct lemon juices.

Unit Mean ± SD Range of variation AIJN proposal Values outside (%)

m M
Titratable acidity at pH 8.1 g/L 52.4 ± 6.9 35.1–65.6 44.8–62.0 15.38 8.79
Citric acid g/L 53.8 ± 9.0 35.1–84.2 45–63.0 19.78 18.68
D-Isocitric acid mg/L 268.9 ± 73.8 114.0–455.7 230–500 35.16
Citric/Isocitric acid ratio – 214.8 ± 68.3 117.0–466.4 Max. 200 49.45
L-Malic acid g/L 1.8 ± 0.9 1.0–4.4 1–7.5
D-Malic acid mg/L NP NP
Ash g/L 2.6 ± 0.6 1.2–5 2.2–4.3 17.58 1.10
Sodium (Na) mg/L 23.1 ± 20.1 3–98.4 Max. 30 25.27
Potassium (K) mg/L 1264.2 ± 267.8 673.6–1953.8 1100–2000 25.27
Magnesium (Mg) mg/L 92.6 ± 20.4 37.5–136.7 70–120 16.48 6.59
Calcium (Ca) mg/L 112.0 ± 43.8 46.8–278.4 45–160 10.99
Total phosphorus (P) mg/L 306.0 ± 73.7 182.7–694.7 80–150 12.09 4.40
Sulphate (SO4) mg/L 27.47 ± 9.89 10–56 Max. 100
Flavanoid-Hesperidin mg/L 364.88 ± 67.26 257–484.82 Max. 1500
Water soluble pectins mg/L 324.34 ± 94.95 164.8–550 Max. 700
Glucose g/L 7.9 ± 2.1 3–15.7 3–12 3.30
Fructose g/L 7.3 ± 1.8 3.4–13.6 3–11 3.30
Glucose/Fructose – 1.1 ± 0.2 0.6–1.6 0.95–1.3 43.75 31.25
Sucrose g/L 4.5 ± 2.2 1–15 Max. 7.0 13.19

SD, standard deviation; AIJN, Association of the Industry of Juices and Nectars of the European Union (EU); NP, not present; m, minimum; M, maximum.

Table 4
Other quality parameters and further criteria for evaluation of identity and authenticity of reconstituted lemon juices.

Unit Mean ± SD Range of variation AIJN proposal Values outside (%)

m M
Titratable acidity at pH 8.1 g/L 52.4 ± 6.6 38.4–78.1 44.8–62.0 13.19 5.49
Citric acid g/L 53.4 ± 10.8 34.2–67.4 45–63.0 12.09 4.40
D-Isocitric acid mg/L 258.7 ± 66.6 138.1–396.4 230–500 42.86
Citric/Isocitric acid ratio – 217.8 ± 63.1 125.2–362.2 Max. 200 51.65
L-Malic acid g/L 1.8 ± 1.0 0.5–5.0 1–7.5 10.99
D-Malic acid mg/L NP NP
Ash g/L 3.0 ± 0.5 1.4–3.9 2.2–4.3 6.59
Sodium (Na) mg/L 51.6 ± 54.4 6.8–220.4 Max. 30 46.15
Potassium (K) mg/L 1313.6 ± 246.1 398.5–2067.6 1100–2000 10.99 2.20
Magnesium (Mg) mg/L 105.5 ± 30.9 57.0–198.8 70–120 10.99 18.68
Calcium (Ca) mg/L 167.9 ± 109.6 56.4–489.8 45–160 32.97
Total phosphorus (P) mg/L 312.7 ± 65.2 164.8–606.4 80–150 10.99 2.20
Sulphate (SO4) mg/L 37.73 ± 13.88 23.16–67.40 Max. 100
Flavanoid-Hesperidin mg/L 367.03 ± 91.57 238.9–550.9 Max. 1500
Water soluble pectins mg/L 293.20 ± 77.75 152.4–405.6 Max. 700
Glucose g/L 8.1 ± 2.0 1.0–15.5 3–12 1.10 4.40
Fructose g/L 7.5 ± 1.3 3–13 3–11 2.20
Glucose/Fructose – 1.1 ± 0.1 0.8–1.3 0.95–1.3 18.75
Sucrose g/L 3.4 ± 1.6 0.5–10.5 Max. 7.0 2.20

SD, standard deviation; AIJN, Association of the Industry of Juices and Nectars of the European Union (EU); NP, not present; m, minimum; M, maximum.

study, a 49.5% and a 51.7% of the citric acid/isocitric acid ratios in
direct and reconstituted juices were higher than the maximum
limit established in the reference guideline. Moreover, values
above 240 were observed either in direct (maximum value:
466.4) or reconstituted (maximum value: 362.2) Spanish lemon
juices.
The ash that represents the total mineral content of lemon juice
was between 2.6 and 3 g/L. The predominant mineral in lemon
juice was potassium (K) (1264.2 and 1313.6 mg/L in direct and
reconstituted juices, respectively), followed by phosphorus (P),
calcium (Ca), magnesium (Mg), and sodium (Na). Potassium values
exceeding the upper limit of the established range (1100–2000 mg/
L) are not found and only a few Italian juices remained slightly
below the lower limit of the range (AIJN, 2013). In this study a
25.3% of results for potassium in direct lemon juice were also
below the minimum reference value. Levels of sodium and calcium
above the respective upper limits occurred especially in the 25.3%
and 11% of direct juice samples. In reconstituted juice, the 46.15%
and 33% of results obtained for sodium and calcium were higher
than the respective maximum limits established in the reference
guideline. According to AIJN (2013), sodium values higher than
30 mg/L can occasionally be found in lemon juices originating from
Southern Spain as a result of fluctuating sodium levels in the irri-
gation water. Extremely high values up to 98.4 mg/L in direct
juices and 220.4 mg/L in reconstitutes were determined herein.
Glucose, fructose and sucrose were detected and quantified in
all juices tested. The presence of sucrose in direct and reconsti-
tuted lemon juices was low: 4.5 and 3.4 g/L, respectively. The
13.19% of results for sucrose in direct juice were higher than the
maximum limit proposed by AIJN (2013). Glucose content was
similar in both type of juice (7.9 and 8.1 g/L) and happened the
same with the fructose content (7.3 and 7.5 g/L). The glucose/fruc-
tose ratio varied between 0.6 and 1.6 in direct juice and there were
big differences with the AIJN range of variation. Almost half of
190 J. Lorente et al. / Food Chemistry 162 (2014) 186–191

Table 5
Formol number and levels of free amino acids in direct lemon juices from Spanish lemons.

Unit Mean ± SD Range of variation AIJN proposal Values outside (%)

m M
Formol number mL NaOH 0.1 N/100 mL 17.5 ± 4.0 10–33 13–26 8.8 2.20
Amino acids
Aspartic acid mmol/L 3.34 ± 1.05 2–5.36 2.26–6.02 15
Threonine mmol/L 0.13 ± 0.05 0.08–0.22 0.08–0.25
Serine mmol/L 1.32 ± 0.25 0.9–2 1.29–3.52 55
Asparagine mmol/L 1.64 ± 0.79 0.95–2.99 0.99–4.55 5
Glutamic acid mmol/L 1.65 ± 0.51 1.01–2.89 1.09–2.72 10 5
Glutamine mmol/L 0.06 ± 0.09 0–0.22 Max. 0.31
Proline mmol/L 2.32 ± 1.45 0.86–5.26 0.87–6.96 10
Glycine mmol/L 0.12 ± 0.05 0.05–0.22 0.09–0.33 20
Alanine mmol/L 0.94 ± 0.26 0.61–1.80 0.90–2.92 35
Valine mmol/L 0.15 ± 0.09 0.06–0.35 0.07–0.30 15 10
Methionine mmol/L 0.01 ± 0.01 0–0.03 Max. 0.03
Iso-leucine mmol/L 0.04 ± 0.01 0.02–0.06 0.02–0.08
Leucine mmol/L 0.05 ± 0.01 0.02–0.07 0.02–0.08
Tyrosine mmol/L 0.02 ± 0.02 0–0.05 Max. 0.04 15
Phenylalanine mmol/L 0.14 ± 0.08 0.03–0.25 0.05–0.24 15 10
Lysine mmol/L 0.09 ± 0.05 0.03–0.20 0.03–0.14 10
Histidine mmol/L 0.02 ± 0.02 0–0.05 Max. 0.07
Arginine mmol/L 0.26 ± 0.13 0–0.45 Max. 0.58

SD, standard deviation; AIJN, Association of the Industry of Juices and Nectars of the European Union (EU); m, minimum; M, maximum.

Table 6
Formol number and levels of free amino acids in reconstituted lemon juices from Spanish lemons.

Unit Mean ± SD Range of variation AIJN proposal Values outside (%)

m M
Formol number mL NaOH 0.1 N/100 mL 19.3 ± 4.1 9.4–29.7 13–26 2.20 5.49
Amino acids
Aspartic acid mmol/L 3.05 ± 1.43 1.10–5.13 2.26–6.02 15
Threonine mmol/L 0.17 ± 0.06 0.09–0.29 0.08–0.25 10
Serine mmol/L 1.11 ± 0.32 0.56–1.92 1.29–3.52 80
Asparagine mmol/L 1.54 ± 0.84 0.74–3.08 0.99–4.55 20
Glutamic acid mmol/L 1.43 ± 0.65 0.47–2.37 1.09–2.72 30
Glutamine mmol/L 0.09 ± 0.09 0–0.29 Max. 0.31
Proline mmol/L 2.37 ± 1.27 1.16–4.55 0.87–6.96 4.35
Glycine mmol/L 0.1 ± 0.05 0.03–0.20 0.09–0.33 50
Alanine mmol/L 0.83 ± 0.23 0.45–1.20 0.90–2.92 55
Valine mmol/L 0.13 ± 0.08 0.04–0.30 0.07–0.30 25
Methionine mmol/L 0.01 ± 0.01 0–0.03 Max. 0.03
Iso-leucine mmol/L 0.04 ± 0.02 0.01–0.07 0.02–0.08 10
Leucine mmol/L 0.04 ± 0.02 0.01–0.07 0.02–0.08 15
Tyrosine mmol/L 0.02 ± 0.02 0–0.05 Max. 0.04 20
Phenylalanine mmol/L 0.13 ± 0.07 0.04–0.27 0.05–0.24 10 15
Lysine mmol/L 0.09 ± 0.05 0.02–0.20 0.03–0.14 10 15
Histidine mmol/L 0.02 ± 0.02 0–0.05 Max. 0.07
Arginine mmol/L 0.27 ± 0.11 0.10–0.51 Max. 0.58

SD, standard deviation; AIJN, Association of the Industry of Juices and Nectars of the European Union (EU); m, minimum; M, maximum.

results (43.8%) were below the minimum established limit for the
glucose/fructose ratio, while a 31.3% was above the upper refer-
ence value.
On the other hand, flavanones are the dominant flavonoid class
in the genus citrus. The flavanone profile of lemons is dominated
by hesperidin and eriocitrin and similar to sweet oranges
(Peterson et al., 2006). Hesperidin was found in a concentration
of 364.88 and 367.03 mg/L in direct and reconstituted juices. The
hesperidin levels were bigger than those reported by other authors
previously (Barreca, Bellocco, Caristi, Leuzzi, & Gattuso, 2011;
Gironés-Vilaplana, Mena, García-Viguera, & Moreno, 2012;
González-Molina et al., 2008, 2009a, 2009b; Xu et al., 2008). This
difference maybe is due to the juice extraction method. In all stud-
ies, the juices were manually obtained unlike of the industrial form
used herein.
The formol number, or formol titration, is merely an index
which reflects the amount of free amino acids. This index and
the complete amino acid profile of direct and reconstituted Spanish
lemon juices are shown in Tables 5 and 6. The formol number was
17.5 and 19.3 mL NaOH 0.1 N/100 mL in direct and reconstituted
juices, respectively. The amino acids found in major level were,
in decreasing order, aspartic acid > proline > glutamic acid > aspar-
agine > serine > alanine; threonine, glutamine, glycine, valine,
methionine, iso-leucine, leucine, tyrosine, phenylalanine, lysine,
histidine and arginine were found at minimal levels. According to
the AIJN guideline for lemon juice, the distribution of the individ-
ual amino acids is influenced neither by the fruit variety nor by
the provenance, except for proline. In the present study, however,
the 55% and the 35% of results for serine and alanine are below the
minimum values established for these amino acids in the reference
guideline. These percentages increased to 80% and 55% in lemon
juices reconstituted from concentrates. Contradicting, the upper
range limit for serine and alanine may be slightly exceeded in some
cases (AIJN, 2013).
 J. Lorente et al. / Food Chemistry 162 (2014) 186–191
4. Conclusions
The complete chemical profile was determined in direct and
reconstituted lemon juice samples to make an authenticity control
guide of commercial juice obtained from the Spanish lemon
varieties ‘Verna’ and ‘Fino’. Results were compared with the AIJN
generic guideline for lemon juice that establishes the chemical pro-
file for various types and origins of fruit of industrial significance.
Our results show that in the Spanish lemon juices there are
parameters that did not reach or exceeded the limits proposed
by AIJN. In addition, the concentration process did not contribute
to vary the juice composition. Therefore, it is important to consider
the change in any of these parameters because it is demonstrated
that high quality juices would not be accepted in view of the exist-
ing guideline.
Acknowledgement
The authors are grateful to AILIMPO (Asociación Interprofesion-
al de Limón y Pomelo, Murcia) for its contribution to the supply of
lemons from different locations during the three growing seasons
covered by this study and the economic cost of chemical analyses.
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